Analysis of low content drug tablets by transmission near infrared spectroscopy: Selection of calibration ranges according to multivariate detection and quantitation limits of PLS models

Alcalà, Manel; Leon, J.; Ropero, Jorge; Blanco, M.; Romañach, Rodolfo J.

doi:10.1002/jps.21373

Cited by 56 publications

(22 citation statements)

References 13 publications

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“…The future calibration model should include spectral bands of the analytes being measured, such as API spectral bands in drug concentration methods. A number of calibration models have been developed using the entire NIR spectrum [43], while other calibration models have been developed using limited spectral regions [44,45]. Thus, there is no set guideline or recommendation to the spectral range that should be used in the calibration model but it is generally recognized that it should include spectral bands related to the analyte.…”

Section: Obtaining Spectra and Selection Of Samples For The Calibratimentioning

confidence: 99%

A Procedure for Developing Quantitative Near Infrared (NIR) Methods for Pharmaceutical Products

Romañach

Román-Ospino

Alcalà

2016

Methods in Pharmacology and Toxicology

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The pharmaceutical industry uses procedures to describe all the instructions needed to perform a process in a consistent manner. Procedures are based on process knowledge and the desire to consistently meet desired specifications. This chapter proposes a procedure for the development of NIR partial least squares (PLS) calibration models for pharmaceutical applications. The chapter captures the lessons learned for more than a decade in studies where NIR spectroscopy has been used for quantitative determinations of drug concentration, moisture, polymorphs, and other important applications. Two examples of recent initiatives to develop NIR calibration models in a more efficient manner reducing the number of calibration samples are also discussed. The procedure differs from previously published guidelines since it is based on specific examples of method validations for pharmaceutical processes and provides clear instructions for method development and validation. The procedure and tutorial should advance the implementation of near infrared spectroscopic (NIRS) quantitative methods in the pharmaceutical industry.

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Section: Obtaining Spectra and Selection Of Samples For The Calibratimentioning

confidence: 99%

A Procedure for Developing Quantitative Near Infrared (NIR) Methods for Pharmaceutical Products

Romañach

Román-Ospino

Alcalà

2016

Methods in Pharmacology and Toxicology

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“…15 Even though the bands they measured in the spectra were broader than those in most OP/FT-IR measurements, they concluded that the selection of wide concentration ranges was not recommended for the determination of analytes at minor levels, even when the concentration of the analyte is within the range of the model.…”

Section: Introductionmentioning

confidence: 96%

Using Multiple Calibration Sets to Improve the Quantitative Accuracy of Partial Least Squares (PLS) Regression on Open-Path Fourier Transform Infrared (OP/FT-IR) Spectra of Ammonia over Wide Concentration Ranges

et al. 2011

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The use of multiple calibration sets in partial least squares (PLS) regression was proposed to improve the quantitative determination of NH 3 over wide concentration ranges from open-path Fourier transform infrared (OP/FT-IR) spectra. The spectra were measured near animal farms, where the path-integrated concentration of NH 3 can fluctuate from nearly zero to as high as approximately 1000 ppm-m. PLS regression with a single calibration set did not cover such a large concentration range effectively, and the quantitative accuracy was degraded due to the nonlinear relationship between concentration and absorbance for spectra measured at low resolution (1 cm À1 and poorer.) In PLS regression with multiple calibration sets, each calibration set covers a part of the entire concentration range, which significantly decreases the serious nonlinearity problem in PLS regression occurring when only a single calibration set is used. The relative error was reduced from approximately 6% to below 2%, and the best results were obtained with four calibration sets, each covering one quarter of the entire concentration range. It was also found that it was possible to build the multiple calibration sets easily and efficiently without extra measurements.

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“…"Green methods" as infrared spectroscopy has become an attractive alternative because they provide accurate results and a low sample preparation time. Near infrared using reflectance accessory (NIRA) has been extensively used in quality control of finished pharmaceuticals and monitoring processes in combination with multivariate regression methods as Partial Least Squares (PLS) (Roggo et al, 2007;Alcalà et al, 2008;Souza et al, 2012;Pan et al, 2014;Wood et al, 2016).…”

Section: Introductionmentioning

confidence: 99%

Simultaneous determination of valsartan, amlodipine besylate and hydrochlorothiazide in tablets by near infrared

Becker¹,

Foresti²,

Almeida³

et al. 2017

J App Pharm Sci

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Interval partial least-squares calibration (iPLS) and synergical partial least-squares calibration (siPLS) methods in combination with near infrared spectroscopy coupled with integrating sphere (NIRA) have been developed for simultaneous determination of amlodipine (AML), valsartan (VAL) and hydrochlorothiazide (HCT) in raw material powder mixtures used for production commercial pharmaceutical product (tablets). Variable selection methods (iPLS and siPLS) were applied to select a spectral range that provided significant information and models with lower prediction errors. A near-infrared reflectance accessory (NIRA) was used for direct sample analysis. Spectral data were acquired between 10000 -4000 cm -1 and divided into 32 intervals. A relative standard error of prediction of 1.27% for VAL, 1.92% for HCT and 5.19% for AML was obtained after selection of better intervals by siPLS. Results shown that variable selection methods associated to NIRA is a relatively simple, free solvent and non-destructive procedure that could be applied to the simultaneous determination of AML, VAL and HCT in tablets.

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Analysis of low content drug tablets by transmission near infrared spectroscopy: Selection of calibration ranges according to multivariate detection and quantitation limits of PLS models

Cited by 56 publications

References 13 publications

A Procedure for Developing Quantitative Near Infrared (NIR) Methods for Pharmaceutical Products

A Procedure for Developing Quantitative Near Infrared (NIR) Methods for Pharmaceutical Products

Using Multiple Calibration Sets to Improve the Quantitative Accuracy of Partial Least Squares (PLS) Regression on Open-Path Fourier Transform Infrared (OP/FT-IR) Spectra of Ammonia over Wide Concentration Ranges

Simultaneous determination of valsartan, amlodipine besylate and hydrochlorothiazide in tablets by near infrared

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